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2-[[(2,3-Difluorophenyl)methyl]thio]-4,6-pyrimidinediamine → 2-[[(2,3-Difluorophenyl)methyl]thio]-5-nitroso4,6-pyrimidinediamine

HRID 968232
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인쇄 미리보기

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HRID 968232 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[N:16]=[C:15]([NH2:17])[CH:14]=[C:13]([NH2:18])[N:12]=1.[N:19]([O-])=[O:20].[Na+]>C(O)(=O)C.O>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[N:12]=[C:13]([NH2:18])[C:14]([N:19]=[O:20])=[C:15]([NH2:17])[N:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 174102292-[[(2,3-Difluorophenyl)methyl]thio]-4,6-pyrimidinediamineHCID 23668193Sodium Nitrite

생성물 1

HCID 222884992-[[(2,3-Difluorophenyl)methyl]thio]-5-nitroso4,6-pyrimidinediamine수율 153.7%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
5 °C

실험 절차

The product of example 5, step (a) (2.5 g) was dissolved in acetic acid (150 ml) and the solution cooled to 5° C. A solution of sodium nitrite (625 mg) in water (50 ml) was added dropwise resulting in a dark blue colouration. The reaction was stirred at room temperature for 30 minutes during which time a pink solid precipitated from solution. This was isolated by filtration and washed with water, then dried at 50° C. to give the sub-titled product as a blue solid (4.14 g)

후처리

  1. customresulting in a dark blue colouration
  2. customprecipitated from solution
  3. customThis was isolated by filtration
  4. washwashed with water
  5. customdried at 50° C.

출처 및 근거

ORD 기록
ord-f2d2073dac2541658b79442bd5aeca75
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06958344B2

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